A purification device for hexafluorobutadiene and its usage method

By installing trays on the sidewall of the distillation column and using locking components, the problem of inconvenient replacement of the high-efficiency adsorbent was solved, enabling efficient purification and high-purity production of hexafluorobutadiene.

CN118767463BActive Publication Date: 2025-11-14FU JIAN SHENG JIAN YANG JIN SHI FU YE YOU XIAN GONG SI
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Patent Information

Application Number
CN202410921729.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-10
Publication Date
2025-11-14
Estimated Expiration
2044-07-10

AI Technical Summary

Technical Problem

In the preparation of high-purity hexafluorobutadiene, the replacement of the high-efficiency adsorbent is inconvenient and takes a long time.

Method used

Design a hexafluorobutadiene purification device with trays located on the side wall of a distillation column. The trays can be quickly installed and disassembled using locking components, and the impurity removal efficiency can be improved by combining a filter screen and scraper structure.

Benefits of technology

It enables rapid replacement of highly efficient adsorbents and the production of high-purity hexafluorobutadiene, thereby improving production efficiency and product purity.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of fine chemical technology, and more particularly to a purification device for hexafluorobutadiene, comprising a distillation column. The distillation column has multiple openings on its sidewall that communicate with the interior, and trays are slidably and sealingly inserted into these openings. Mounting blocks are fixedly installed on the surface of each tray, and locking openings are provided on the surface of each mounting block. Multiple sets of locking components are fixedly installed on the sidewall of the distillation column, each set used to lock multiple trays. Each locking component includes a fixing block fixedly installed on the sidewall of the distillation column, with a through-hole on its surface. A locking rod is vertically and slidably inserted into the through-hole, and a pull plate is fixedly installed at the bottom end of the locking rod. A first telescopic spring is sleeved on the locking rod. Trays for holding high-efficiency adsorbents are located on the sidewall of the distillation column, and the locking components allow for rapid installation and removal of the trays, improving the efficiency of replacing high-efficiency adsorbents.
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Description

Technical Field

[0001] This invention relates to the field of fine chemical technology, and in particular to a purification device for hexafluorobutadiene and its method of use. Background Technology

[0002] Hexafluorobutadiene electronic gas is a dry etching gas with extremely low greenhouse effect and excellent etching performance. Therefore, it is mainly used in plasma dielectric etching technology for semiconductor products and dry etching of ultra-large-scale integrated circuits. In order to avoid poor precision in etching due to impurities in hexafluorobutadiene, it is necessary to prepare high-purity hexafluorobutadiene through purification equipment.

[0003] In the preparation of high-purity hexafluorobutadiene, hexafluorobutadiene needs to be passed into a distillation column with a high-efficiency adsorbent for distillation. After a long period of use, the high-efficiency adsorbent needs to be replaced. However, since the multiple trays used to hold the high-efficiency adsorbent are usually located inside the distillation column, it is inconvenient and time-consuming to replace the high-efficiency adsorbent. Summary of the Invention

[0004] The purpose of this invention is to address the following shortcomings in the prior art: In the preparation of high-purity hexafluorobutadiene, it is necessary to pass the hexafluorobutadiene into a distillation column with a high-efficiency adsorbent for distillation. However, after a long period of use, the high-efficiency adsorbent needs to be replaced. Since the multiple trays used to hold the high-efficiency adsorbent are generally located inside the distillation column, it is inconvenient and time-consuming to replace the high-efficiency adsorbent. Therefore, this invention proposes a purification device for hexafluorobutadiene and its usage method.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] A purification device for hexafluorobutadiene includes a distillation column, wherein a steam inlet pipe is fixedly installed at the bottom of the distillation column, a steam outlet pipe is fixedly installed at the top of the distillation column, a liquid inlet pipe is fixedly installed on the side wall at the top of the distillation column, and multiple openings communicating with the interior are provided on the side wall of the distillation column, wherein a tray is slidably and sealedly inserted into the opening.

[0007] An mounting block is fixedly installed on the surface of the tray, and a locking port is opened on the surface of the mounting block. Multiple sets of locking components are fixedly installed on the side wall of the distillation column. The multiple sets of locking components are used to lock multiple trays respectively. The locking component includes a fixing block fixedly installed on the side wall of the distillation column. A through hole is opened on the surface of the fixing block. A locking rod is vertically slidably inserted into the through hole. A pull plate is fixedly installed at the bottom end of the locking rod. A first telescopic spring is sleeved on the locking rod. The two ends of the first telescopic spring are fixedly connected to the pull plate and the fixing block respectively. The multiple locking rods correspond to the positions of multiple locking ports respectively.

[0008] The pull plate surface is provided with an adsorption assembly for adsorbing mounting blocks. The adsorption assembly includes a first hollow rod fixedly mounted on the upper surface of the pull plate and a suction cup fixedly mounted on the top of the first hollow rod. Multiple suction cups are located below multiple mounting blocks. The pull plate surface has a rotating opening communicating with the first hollow rod. A rotating shaft is rotatably mounted within the rotating opening. One end of the rotating shaft, located inside the first hollow rod, is fixedly mounted with an arc-shaped plate via a connecting rod. The first hollow rod surface has an arc-shaped air inlet, which is sealed by the arc-shaped plate. The bottom end of the rotating shaft is fixedly mounted with... The device includes a rotating block, a torsion spring fitted on the rotating shaft, and two ends of the torsion spring fixedly connected to the rotating block and the pull plate, respectively. A filter screen is fixedly installed inside the liquid inlet pipe, and a circular opening is provided at the center of the filter screen. A second hollow rod with a closed end is rotatably installed inside the circular opening. A plug rod is slidably inserted inside the second hollow rod, and a second telescopic spring is provided inside the second hollow rod. The two ends of the second telescopic spring are fixedly connected to the plug rod and the second hollow rod, respectively. Scraper strips are symmetrically fixedly installed on the surface of the second hollow rod, and both scraper strips are in sliding contact with the filter screen. The rotation of the second hollow rod is controlled by a pressing component.

[0009] Preferably, the pressure assembly includes a reciprocating screw horizontally rotatably mounted inside the inlet pipe, a slider threaded onto the reciprocating screw, two symmetrically fixed abutment rods and a first abutment plate fixedly mounted on the surface of the slider, a spring rod fixedly mounted at one end of the reciprocating screw, the first abutment plate fixedly mounted at one end of the spring rod, and a second abutment plate fixedly mounted at one end of the insert rod. The positions of the first abutment plate and the second abutment plate correspond to each other. The slider is restricted from rotation by a limiting component. The ends of the two abutment rods correspond to the surface positions of the first abutment plate. The reciprocating screw is controlled to rotate by a transmission assembly.

[0010] Preferably, the limiting component includes a limiting groove horizontally formed on the inner wall of the inlet pipe and a limiting rod fixedly installed on the lower surface of the slider, with the bottom end of the limiting rod slidably disposed within the limiting groove.

[0011] Preferably, the transmission assembly includes a rotating rod and a rotating blade fixedly sleeved on the rotating rod. A rotating ring is rotatably sleeved on the rotating rod. Support rods are symmetrically fixedly installed on the outer ring wall of the rotating ring. One end of each of the two support rods is fixedly connected to the inner wall of the liquid inlet pipe. One end of the rotating rod is fixedly connected to one end of the reciprocating lead screw.

[0012] Preferably, a spherical groove is provided at one end of the abutment rod near the first abutment plate, and a rolling ball is embedded in the spherical groove.

[0013] Preferably, the second hollow rod has a vent at one closed end, and a vent pipe is fixedly installed inside the vent. The insertion rod is slidably inserted into the second hollow rod. A disc is fixedly installed inside the liquid inlet pipe through two connecting blocks. An air chamber is opened inside the disc. The vent pipe is rotatably connected to the disc and communicates with the air chamber. The surface of the disc has multiple mounting ports corresponding to the positions of multiple filter holes on the filter screen surface. A corrugated pipe with a closed end is fixedly installed inside each mounting port. A conical cleaning rod is fixedly installed at the closed end of the corrugated pipe. The multiple cleaning rods correspond to the positions of multiple filter holes on the filter screen surface.

[0014] A method for using a purification device for hexafluorobutadiene, the method comprising the following steps:

[0015] S1: The adsorption resin and the aqueous solution of graphene oxide, potassium borohydride and water are stirred and mixed in proportion. After filtration and drying, nitrogen gas is introduced and the mixture is calcined and then cooled to room temperature to obtain a high-efficiency adsorbent.

[0016] S2: Pull the tray out from the opening, then put the high-efficiency adsorbent into the tray, push it into the opening, and lock the tray using the locking component.

[0017] S3: The hexafluorobutadiene liquid to be purified is introduced into the distillation column through the inlet pipe, and the steam is introduced into the distillation column through the steam inlet pipe at the bottom of the distillation column. The hexafluorobutadiene liquid will pass through the high-efficiency adsorbent located in multiple trays in sequence, so that the excess impurities in the hexafluorobutadiene liquid can be effectively adsorbed.

[0018] S4: The vapor phase emitted by the steam comes into countercurrent contact with the descending hexafluorobutadiene liquid. During the two-phase contact, the volatile components in the hexafluorobutadiene liquid continuously transfer to the vapor phase, while the non-volatile components in the vapor phase continuously transfer to the hexafluorobutadiene liquid. The closer the vapor phase is to the top of the column, the higher the concentration of its volatile components, while the closer the hexafluorobutadiene liquid is to the bottom of the column, the more concentrated its non-volatile components become, thereby achieving the purpose of component separation.

[0019] S5: The steam carrying the separated components exits the distillation column from the steam outlet pipe at the top of the column and enters the subsequent processing equipment to obtain high-purity hexafluorobutadiene product.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] The trays for placing the high-efficiency adsorbent are located on the side wall of the distillation column. With the help of locking components, the trays can be installed and removed quickly. Compared with the traditional method of replacing the high-efficiency adsorbent inside the distillation column, it is more convenient and efficient to replace the high-efficiency adsorbent by pulling the trays out from the outside.

[0022] The filter screen inside the liquid inlet pipe can remove some solid impurities and components that are not easy to distill from the liquid hexafluorobutadiene, thereby improving the purity of the hexafluorobutadiene product after distillation.

[0023] When the hexafluorobutadiene liquid enters the inlet pipe, the two scrapers will intermittently slide and contact the surface of the filter screen, thereby cleaning the impurities accumulated on the surface of the filter screen and preventing the accumulation of impurities from affecting the water permeability of the filter screen.

[0024] When the scraper rotates, multiple cleaning rods also move and insert themselves into multiple filter holes on the filter screen surface, thereby cleaning impurities located in the filter holes, enhancing the overall cleaning of the filter screen, and improving the cleaning effect. Attached Figure Description

[0025] Figure 1 This is a frontal three-dimensional structural diagram of a purification device for hexafluorobutadiene proposed in this invention;

[0026] Figure 2 This is a three-dimensional back view of the purification device for hexafluorobutadiene proposed in this invention.

[0027] Figure 3 This is a three-dimensional structural diagram of the distillation column in the purification device for hexafluorobutadiene proposed in this invention;

[0028] Figure 4 This is a partial three-dimensional structural diagram of the tray in the purification device for hexafluorobutadiene proposed in this invention.

[0029] Figure 5 This is a partial three-dimensional structural diagram of the locking component and the adsorption component in the purification device for hexafluorobutadiene proposed in this invention.

[0030] Figure 6 This is a schematic diagram of a partial three-dimensional cross-sectional structure of the inlet pipe in a purification device for hexafluorobutadiene proposed in this invention.

[0031] Figure 7 This is a partial three-dimensional structural diagram of the transmission component and the pressure component in the purification device for hexafluorobutadiene proposed in this invention.

[0032] Figure 8 This is a partial three-dimensional structural diagram of the filter screen in a purification device for hexafluorobutadiene proposed in this invention;

[0033] Figure 9 for Figure 4 Enlarged structural diagram at point A in the middle;

[0034] Figure 10 for Figure 5Enlarged structural diagram at point B;

[0035] Figure 11 for Figure 7 Enlarged structural diagram at point C.

[0036] In the diagram: 1. Distillation column, 2. Steam inlet pipe, 3. Steam outlet pipe, 4. Liquid inlet pipe, 5. Port, 6. Tray, 7. Locking port, 8. Locking rod, 9. Pull plate, 10. First telescopic spring, 11. First hollow rod, 12. Suction cup, 13. Rotating shaft, 14. Arc plate, 15. Gas inlet, 16. Torsion spring, 17. Filter screen, 18. Second hollow rod, 19. Insert rod, 20. Second telescopic spring, 21. Scraper, 22. Reciprocating screw, 23. Slider, 24. Abutment rod, 25. First abutment plate, 26. Spring rod, 27. Second abutment plate, 28. Limiting groove, 29. Limiting rod, 30. Rotating rod, 31. Rotating blade, 32. Rotating ring, 33. Rolling ball, 34. Gas guide pipe, 35. Disc, 36. Bellows, 37. Orifice cleaning rod. Detailed Implementation

[0037] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0038] Reference Figures 1-11 A purification device for hexafluorobutadiene includes a distillation column 1, a steam inlet pipe 2 fixedly installed at the bottom of the distillation column 1, a steam outlet pipe 3 fixedly installed at the top of the distillation column 1, a liquid inlet pipe 4 fixedly installed on the side wall at the top of the distillation column 1, and multiple openings 5 ​​connected to the interior of the distillation column 1 on the side wall, with a tray 6 slidably and sealed inside the openings 5.

[0039] A mounting block is fixedly installed on the surface of the tray 6. The mounting block has a locking port 7. Multiple sets of locking components are fixedly installed on the side wall of the distillation column 1. The multiple sets of locking components are used to lock multiple trays 6. The locking components include a fixing block fixedly installed on the side wall of the distillation column 1. The fixing block has a through hole. A locking rod 8 is vertically slidably inserted into the through hole. A pull plate 9 is fixedly installed at the bottom of the locking rod 8. A first telescopic spring 10 is sleeved on the locking rod 8. The two ends of the first telescopic spring 10 are fixedly connected to the pull plate 9 and the fixing block, respectively. The multiple locking rods 8 correspond to the positions of multiple locking ports 7.

[0040] When it is necessary to replace the high-efficiency adsorbent located in the tray 6, first pull down the pull plate 9 to control the end of the locking rod 8 to move out of the locking port 7, thereby releasing the lock on the tray 6. Then, control the tray 6 to move out of the through port 5, and then replace the high-efficiency adsorbent located inside it. After the replacement is completed, push the tray 6 to move it back into the through port 5. At this time, the locking port 7 will correspond to the position of the locking rod 8. Then release the locking rod 8, and the locking rod 8 will quickly move upward and reset under the elastic potential energy of the first extension spring 10, and the top end will insert into the locking port 7, thereby completing the locking of the tray 6 again.

[0041] The surface of the pull plate 9 is provided with an adsorption assembly for adsorbing the mounting blocks. The adsorption assembly includes a first hollow rod 11 fixedly installed on the upper surface of the pull plate 9 and a suction cup 12 fixedly installed on the top of the first hollow rod 11. Multiple suction cups 12 are located below multiple mounting blocks respectively. The surface of the pull plate 9 has a rotating port that communicates with the first hollow rod 11. A rotating shaft 13 is rotatably installed in the rotating port. One end of the rotating shaft 13 located inside the first hollow rod 11 is fixedly installed with an arc-shaped plate 14 through a connecting rod. The surface of the first hollow rod 11 has an arc-shaped air inlet 15. The arc-shaped plate 14 is used to close the air inlet 15. A rotating block is fixedly installed at the bottom end of the rotating shaft 13. A torsion spring 16 is sleeved on the rotating shaft 13. The two ends of the torsion spring 16 are fixedly connected to the rotating block and the pull plate 9 respectively.

[0042] When the locking rod 8 rapidly moves upward and resets under the elastic potential energy of the first telescopic spring 10, and its end inserts into the locking port 7, the first hollow rod 11 also moves upward along with the suction cup 12. The suction cup 12 abuts against the mounting block above it, and the suction cup 12 deforms under the pressure. The gas inside the suction cup 12 then escapes from the gap between itself and the mounting block, thus completing the adsorption and enhancing the locking effect of the tower plate 6. When it is necessary to release the lock on the tower plate 6, it is necessary to... First, control the rotating shaft 13 to rotate so that the arc plate 14 no longer covers the air inlet 15. At this time, the gas in the outside will enter the first hollow rod 11 from the air inlet 15, thereby releasing the adsorption between the suction cup 12 and the mounting block. Then, control the locking rod 8 to move down so that the end of the locking rod 8 can be removed from the locking port 7. When the rotating shaft 13 is released, the rotating shaft 13 will quickly rotate and reset the arc plate 14 under the elastic potential energy of the torsion spring 16, and the arc plate 14 will cover the air inlet 15 again.

[0043] A filter screen 17 is fixedly installed inside the liquid inlet pipe 4. The filter screen 17 can remove some solid impurities and components that are not easy to distill from the hexafluorobutadiene liquid, thereby improving the purity of the hexafluorobutadiene product after distillation. A circular opening is provided at the center of the filter screen 17. A second hollow rod 18 with a closed end is rotatably installed inside the circular opening. An insert rod 19 is slidably inserted inside the second hollow rod 18. A second telescopic spring 20 is provided inside the second hollow rod 18. The two ends of the second telescopic spring 20 are fixedly connected to the insert rod 19 and the second hollow rod 18, respectively. Scrapers 21 are symmetrically fixedly installed on the surface of the second hollow rod 18. Both scrapers 21 are in sliding contact with the filter screen 17. The rotation of the second hollow rod 18 is controlled by a pressing component.

[0044] The pressure assembly includes a reciprocating screw 22 horizontally rotatably installed inside the inlet pipe 4, a slider 23 threaded onto the reciprocating screw 22, two abutment rods 24 symmetrically fixedly installed on the surface of the slider 23, and a first abutment plate 25. A spring rod 26 is fixedly installed at one end of the reciprocating screw 22, the first abutment plate 25 is fixedly installed at one end of the spring rod 26, and a second abutment plate 27 is fixedly installed at one end of the insertion rod 19. The positions of the first abutment plate 25 and the second abutment plate 27 correspond to each other. The slider 23 is restricted from rotating by a limiting component, which includes a limiting groove 28 horizontally opened on the inner wall of the inlet pipe 4 and a limiting rod 29 fixedly installed on the lower surface of the slider 23. The bottom end of the limiting rod 29 is slidably disposed in the limiting groove 28. The ends of the two abutment rods 24 correspond to the surface positions of the first abutment plate 25. The reciprocating screw 22 is controlled to rotate by a transmission assembly.

[0045] The transmission assembly includes a rotating rod 30 and a rotating blade 31 fixedly sleeved on the rotating rod 30. A rotating ring 32 is rotatably sleeved on the rotating rod 30. Support rods are symmetrically fixedly installed on the outer ring wall of the rotating ring 32. One end of each support rod is fixedly connected to the inner wall of the liquid inlet pipe 4. One end of the rotating rod 30 is fixedly connected to one end of the reciprocating screw 22.

[0046] When the hexafluorobutadiene liquid enters the inlet pipe 4, the rotating blade 31 located in the inlet pipe 4 will be driven by the flow force of the liquid, causing the rotating rod 30 and the reciprocating screw 22 to rotate together. At this time, the slider 23 threaded onto the reciprocating screw 22 will move laterally back and forth with the two abutment rods 24 under the restriction of the limiting groove 28 and the limiting rod 29. The two abutment rods 24 will intermittently abut against the first abutment plate 25. When the two abutment rods 24 abut against the first abutment plate 25 and push the first abutment plate 25 towards the second abutment plate 27, the surface of the first abutment plate 25 will slide into contact with the ends of the two abutment rods 24, and the distance between the first abutment plate 25 and the second abutment plate 27 will gradually decrease. When the first abutment plate 25 abuts against the second abutment plate 27, under the action of friction, the second hollow rod 18, the insert rod 19 and The two scraper strips 21 will rotate, scraping off the impurities accumulated on the surface of the filter screen 17. As the first abutment plate 25 moves, the insertion rod 19 will also move inside the second hollow rod 18, and the second telescopic spring 20 will contract. When the two abutment rods 24 move away from the second abutment plate 27, the pressure exerted by the first abutment plate 25 on the second abutment plate 27 will gradually weaken. The first abutment plate 25 will gradually move back to its original position under the elastic potential energy of the spring rod 26, and the insertion rod 19 will also gradually move back to its original position under the elastic potential energy of the second telescopic spring 20 until the first abutment plate 25 no longer abuts against the second abutment plate 27. At this point, the rotation of the first abutment plate 25 will not cause the second abutment plate 27 to rotate. That is, the rotation of the two scraper strips 21 is intermittent, avoiding continuous rotation that would cause severe wear on the scraper strips 21.

[0047] The end of the abutment 24 near the first abutment plate 25 has a spherical groove, and a rolling ball 33 is embedded in the spherical groove.

[0048] The ball 33 can reduce the friction between the contact surfaces of the push rod 24 and the first push plate 25, reduce the wear between the end of the push rod 24 and the first push plate 25, and make the rotation of the first push plate 25 smoother.

[0049] The second hollow rod 18 has a vent at one closed end, and a vent pipe 34 is fixedly installed inside the vent. The insertion rod 19 is slidably inserted into the second hollow rod 18. A disc 35 is fixedly installed inside the liquid inlet pipe 4 through two connecting blocks. The diameter of the disc 35 is smaller than the diameter of the filter screen 17. An air chamber is opened inside the disc 35. The vent pipe 34 is rotatably connected to the disc 35 and communicates with the air chamber. Multiple installation ports are opened on the surface of the disc 35, which correspond to the positions of multiple filter holes on the surface of the filter screen 17. A corrugated pipe 36 with a closed end is fixedly installed inside the installation port. A conical cleaning rod 37 is fixedly installed at the closed end of the corrugated pipe 36. Multiple cleaning rods 37 correspond to the positions of multiple filter holes on the surface of the filter screen 17.

[0050] When the first abutment 25 abuts against the second abutment 27 and moves towards the filter screen 17, the insertion rod 19 moves inside the second hollow rod 18. The volume inside the second hollow rod 18 decreases, and the pressure increases. The gas inside the second hollow rod 18 enters the air chamber through the air guide tube 34. At this time, the multiple corrugated tubes 36 are stretched by the gas, and the multiple cleaning rods 37 are inserted into the multiple filter holes on the surface of the filter screen 17, thereby pushing out the impurities accumulated in the filter holes, strengthening the overall cleaning of the filter screen 17, and improving the cleaning effect of the filter screen 17. When the insertion rod 19 moves and resets, the multiple corrugated tubes 36 will shrink and return to their original position, and the multiple cleaning rods 37 will move out from the multiple filter holes.

[0051] A method for using a purification device for hexafluorobutadiene, comprising the following steps:

[0052] S1: The adsorption resin and the aqueous solution of graphene oxide, potassium borohydride and water are stirred and mixed in proportion. After filtration and drying, nitrogen gas is introduced and the mixture is calcined and then cooled to room temperature to obtain a high-efficiency adsorbent.

[0053] S2: Pull the tray 6 out from the port 5, then put the high-efficiency adsorbent into the tray 6, and then push it into the port 5, and lock the tray 6 by the locking component.

[0054] S3: The hexafluorobutadiene liquid to be purified is introduced into the distillation column 1 through the inlet pipe 4, and the steam is introduced into the distillation column 1 through the steam inlet pipe 2 at the bottom of the distillation column 1. The hexafluorobutadiene liquid will pass through the high-efficiency adsorbent located in multiple trays 6 in sequence, so that the excess impurities in the hexafluorobutadiene liquid can be effectively adsorbed.

[0055] S4: The vapor phase emitted by the steam comes into countercurrent contact with the descending hexafluorobutadiene liquid. During the two-phase contact, the volatile components in the hexafluorobutadiene liquid continuously transfer to the vapor phase, while the non-volatile components in the vapor phase continuously transfer to the hexafluorobutadiene liquid. The closer the vapor phase is to the top of the column, the higher the concentration of its volatile components, while the closer the hexafluorobutadiene liquid is to the bottom of the column, the more concentrated its non-volatile components become, thereby achieving the purpose of component separation.

[0056] S5: The steam carrying the separated components exits the distillation column 1 through the steam outlet pipe 3 at the top and enters the subsequent processing equipment to obtain high-purity hexafluorobutadiene product.

[0057] In this invention, when it is necessary to replace the high-efficiency adsorbent located in the tray 6, firstly, by pulling down the pull plate 9, the end of the locking rod 8 is moved out of the locking port 7, thus releasing the lock on the tray 6. Then, the tray 6 is moved out of the through port 5, and the high-efficiency adsorbent located inside it is replaced. After the replacement is completed, the tray 6 is pushed back into the through port 5. At this time, the locking port 7 will correspond to the position of the locking rod 8. Then, the locking rod 8 is released, and the locking rod 8 will quickly move upward and reset under the elastic potential energy of the first extension spring 10, and its top end will be inserted into the locking port 7, thereby locking the tray 6 again. Compared with the traditional replacement of the high-efficiency adsorbent in the distillation column 1, replacing the high-efficiency adsorbent by pulling the tray 6 from the outside is more convenient and has higher replacement efficiency.

[0058] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A purification apparatus for hexafluorobutadiene, comprising a distillation column (1), characterized in that, The bottom of the distillation column (1) is fixedly installed with a steam inlet pipe (2), the top of the distillation column (1) is fixedly installed with a steam outlet pipe (3), the side wall at the top of the distillation column (1) is fixedly installed with a liquid inlet pipe (4), the side wall of the distillation column (1) is provided with multiple openings (5) that are connected to the interior, and a tray (6) is slidably and sealed inside the opening (5). The tray (6) is fixedly mounted with an installation block. The installation block has a locking port (7) on its surface. The distillation column (1) has multiple sets of locking components fixedly mounted on its side wall. The multiple sets of locking components are used to lock multiple trays (6). The locking components include a fixing block fixedly mounted on the side wall of the distillation column (1). The fixing block has a through hole on its surface. A locking rod (8) is vertically slidably inserted into the through hole. A pull plate (9) is fixedly mounted at the bottom of the locking rod (8). A first telescopic spring (10) is sleeved on the locking rod (8). The two ends of the first telescopic spring (10) are fixedly connected to the pull plate (9) and the fixing block, respectively. The multiple locking rods (8) correspond to the positions of multiple locking ports (7). The surface of the pull plate (9) is provided with an adsorption assembly, which is used to adsorb the mounting blocks. The adsorption assembly includes a first hollow rod (11) fixedly installed on the upper surface of the pull plate (9) and a suction cup (12) fixedly installed on the top of the first hollow rod (11). Multiple suction cups (12) are respectively located below multiple mounting blocks. The surface of the pull plate (9) is provided with a rotating port that communicates with the first hollow rod (11). A rotating shaft (13) is sealed and rotatably installed inside the rotating port. One end of the rotating shaft (13) located inside the first hollow rod (11) is fixedly installed with an arc-shaped plate (14) through a connecting rod. The surface of the first hollow rod (11) is provided with an arc-shaped air inlet (15). The arc-shaped plate (14) is used to close the air inlet (15). A rotating block is fixedly installed at the bottom end of the rotating shaft (13). A torsion spring (16) is sleeved on the shaft (13). The two ends of the torsion spring (16) are fixedly connected to the rotating block and the pull plate (9) respectively. A filter screen (17) is fixedly installed in the liquid inlet pipe (4). A round opening is provided at the center of the filter screen (17). A second hollow rod (18) with a closed end is rotatably installed in the round opening. A plug rod (19) is slidably inserted in the second hollow rod (18). A second telescopic spring (20) is provided in the second hollow rod (18). The two ends of the second telescopic spring (20) are fixedly connected to the plug rod (19) and the second hollow rod (18) respectively. Scrapers (21) are symmetrically fixedly installed on the surface of the second hollow rod (18). Both scrapers (21) are in sliding contact with the filter screen (17). The second hollow rod (18) is controlled to rotate by the pressure assembly.

2. The purification equipment for hexafluorobutadiene according to claim 1, characterized in that, The pressure assembly includes a reciprocating screw (22) horizontally rotatably installed in the inlet pipe (4), a slider (23) threaded onto the reciprocating screw (22), two abutting rods (24) symmetrically fixedly installed on the surface of the slider (23), and a first abutting plate (25). A spring rod (26) is fixedly installed at one end of the reciprocating screw (22), and the first abutting plate (25) is fixedly installed at one end of the spring rod (26). A second abutting plate (27) is fixedly installed at one end of the insert rod (19). The positions of the first abutting plate (25) and the second abutting plate (27) correspond. The slider (23) is restricted from rotation by a limiting component. The ends of the two abutting rods (24) correspond to the surface positions of the first abutting plate (25). The reciprocating screw (22) is controlled to rotate by a transmission assembly.

3. The purification equipment for hexafluorobutadiene according to claim 2, characterized in that, The limiting component includes a limiting groove (28) horizontally opened on the inner wall of the liquid inlet pipe (4) and a limiting rod (29) fixedly installed on the lower surface of the slider (23), with the bottom end of the limiting rod (29) slidably disposed in the limiting groove (28).

4. The purification equipment for hexafluorobutadiene according to claim 2, characterized in that, The transmission assembly includes a rotating rod (30) and a rotating blade (31) fixedly sleeved on the rotating rod (30). A rotating ring (32) is rotatably sleeved on the rotating rod (30). Support rods are symmetrically fixedly installed on the outer ring wall of the rotating ring (32). One end of each of the two support rods is fixedly connected to the inner wall of the liquid inlet pipe (4). One end of the rotating rod (30) is fixedly connected to one end of the reciprocating screw (22).

5. The purification equipment for hexafluorobutadiene according to claim 2, characterized in that, The abutment (24) has a spherical groove at one end near the first abutment plate (25), and a rolling ball (33) is embedded in the spherical groove.

6. The purification equipment for hexafluorobutadiene according to claim 2, characterized in that, The second hollow rod (18) has a vent at one closed end. A vent pipe (34) is fixedly installed inside the vent. The insertion rod (19) is slidably inserted into the second hollow rod (18). A disc (35) is fixedly installed inside the liquid inlet pipe (4) through two connecting blocks. An air chamber is opened inside the disc (35). The vent pipe (34) is rotatably connected to the disc (35) and communicates with the air chamber. Multiple mounting ports are opened on the surface of the disc (35) that correspond to the positions of multiple filter holes on the surface of the filter screen (17). A corrugated pipe (36) with a closed end is fixedly installed inside the mounting port. A conical cleaning rod (37) is fixedly installed at the closed end of the corrugated pipe (36). Multiple cleaning rods (37) correspond to the positions of multiple filter holes on the surface of the filter screen (17).

7. A method of using the purification equipment for hexafluorobutadiene as described in any one of claims 1-6, characterized in that, The method of use includes the following steps: S1: The adsorption resin and the aqueous solution of graphene oxide, potassium borohydride and water are stirred and mixed in proportion. After filtration and drying, nitrogen gas is introduced and the mixture is calcined and then cooled to room temperature to obtain a high-efficiency adsorbent. S2: Pull the tray (6) out from the port (5), then put the high-efficiency adsorbent into the tray (6), and then push it into the port (5), and lock the tray (6) by the locking component. S3: The hexafluorobutadiene liquid to be purified is introduced into the distillation column (1) through the inlet pipe (4), and the steam is introduced into the distillation column (1) through the steam inlet pipe (2) at the bottom of the distillation column (1). The hexafluorobutadiene liquid will pass through the high-efficiency adsorbent located in multiple trays (6) in sequence, so that the excess impurities in the hexafluorobutadiene liquid can be effectively adsorbed. S4: The vapor phase emitted by the steam comes into countercurrent contact with the descending hexafluorobutadiene liquid. During the two-phase contact, the volatile components in the hexafluorobutadiene liquid continuously transfer to the vapor phase, while the non-volatile components in the vapor phase continuously transfer to the hexafluorobutadiene liquid. The closer the vapor phase is to the top of the column, the higher the concentration of its volatile components, while the closer the hexafluorobutadiene liquid is to the bottom of the column, the more concentrated its non-volatile components become, thereby achieving the purpose of component separation. S5: The steam carrying the separated components exits the distillation column (1) through the steam outlet pipe (3) at the top and enters the subsequent processing equipment to obtain high-purity hexafluorobutadiene products.

Citation Information

Patent Citations

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